CN107500772A - A kind of silicon carbide ceramics precast body, aluminum-base silicon carbide ceramic material and preparation method thereof - Google Patents

A kind of silicon carbide ceramics precast body, aluminum-base silicon carbide ceramic material and preparation method thereof Download PDF

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CN107500772A
CN107500772A CN201710620667.5A CN201710620667A CN107500772A CN 107500772 A CN107500772 A CN 107500772A CN 201710620667 A CN201710620667 A CN 201710620667A CN 107500772 A CN107500772 A CN 107500772A
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silicon carbide
precast body
carbide ceramics
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aluminum
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马少杰
杨小猛
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SUZHOU NORETA NEW MATERIAL TECHNOLOGY Co Ltd
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SUZHOU NORETA NEW MATERIAL TECHNOLOGY Co Ltd
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Abstract

The invention discloses a kind of silicon carbide ceramics precast body, aluminum-base silicon carbide ceramic material and preparation method thereof, it is related to material and its preparing technical field, solves the low technical problem of the volume fraction of the low intensity of silicon carbide ceramics precast body prepared by existing preparation technology, structure heterogeneity and carborundum.The present invention main technical schemes be:The raw material for preparing silicon carbide ceramics precast body is well mixed, raw material slurry is made;Preparing the raw material of silicon carbide ceramics precast body includes carborundum, dispersant, organic monomer and water;Initiator is added into raw material slurry, ceramic slurry is obtained after well mixed;Carry out vacuum degassing processing, casting, demoulding drying successively to ceramic slurry, obtain biscuit of ceramics;Biscuit of ceramics is sintered at 800 1200 DEG C, obtains silicon carbide ceramics precast body.The silicon carbide ceramics precast body homogeneous present invention is mainly used for high intensity, structure is prepared, and then prepare high performance aluminum-base silicon carbide ceramic material.

Description

A kind of silicon carbide ceramics precast body, aluminum-base silicon carbide ceramic material and preparation method thereof
Technical field
The present invention relates to technical field of material, more particularly to a kind of silicon carbide ceramics precast body and preparation method thereof, Aluminum-base silicon carbide ceramic material and preparation method thereof.
Background technology
Aluminum-base silicon carbide ceramics (SiCp/Al) composite combines the premium properties of silicon carbide ceramics and aluminium alloy, tool There is the features such as high specific strength, good thermal conductivity, low-expansion coefficient, in fields such as Electronic Packaging, Aero-Space, military affairs, automobiles Have a wide range of applications.The preparation technology of aluminum-base silicon carbide ceramic material mainly whether there is pressure Infiltration Technics and stirring casting technique. Wherein, stirring casting technique is mainly to be continuously added to silicon-carbide particle in the aluminium liquid of melting, and silicon-carbide particle and aluminium are closed Finance is poured into mould after being combined, and obtains aluminum-base silicon carbide billet.Pressureless infiltration technique is mainly by aluminium alloy without pressure Penetrate into silicon carbide ceramics precast body well prepared in advance (that is, porous silicon carbide ceramic material), form aluminum-base silicon carbide pottery Porcelain densified composite.Stirring casting technique can not prepare high body due to silicon-carbide particle and the poor compatibility of aluminium liquid Fraction, high performance aluminum-base silicon carbide material;The saturating technique of pressureless infiltration can realize that aluminum-base silicon carbide " net " size is molded (that is, after aluminum-base silicon carbide shaping, it is only necessary to which a small amount of processing is not reprocessed, it is possible to the forming technique used as component). So pressureless infiltration process is the preferred technique for preparing aluminum-base silicon carbide ceramic material.And silicon carbide ceramics precast body is strong Whether degree, silicon carbide ceramics precast body have the carborundum of high-volume fractional, whether silicon carbide ceramics precursor structure is homogeneous is Whether pressureless infiltration technique can prepare the key factor of high-performance aluminium-base thyrite.
At present, the preparation technology of silicon carbide ceramics precast body (that is, porous silicon carbide ceramic material) mainly has dry-pressing formed Technique and injection molding technique.Wherein, dry pressuring forming process is will to prepare the dry powder blank of silicon carbide ceramics in mould using pressure A kind of forming method of dense body is pressed into type.Injection molding technique mainly includes:Dispensing, mixing (need to add binding agent, feed Material), injection moulding, degreasing and sintering.
But aluminum-base silicon carbide ceramics preparative body low intensity prepared by inventor's discovery dry pressuring forming process, structure are homogeneous Property is poor, can not realize that the later stage prepares the high-performance aluminum base silicon carbide for meeting requirement.Injection molding technique needs substantial amounts of Organic binder bond, biscuit of ceramics shrink big, can not prepare the thyrite (carborundum at present of high-volume fractional 60%) volume fraction is substantially less than, thus can not also realize that the later stage prepares the high-performance aluminium-base carbonization for meeting requirement Silicon ceramic material.
The content of the invention
In view of this, present invention is primarily intended to provide a kind of preparation method of silicon carbide ceramics precast body, prepare strong The silicon carbide ceramics precast body that degree is higher, structure is homogeneous and silicon carbide body fraction is higher.
To reach above-mentioned purpose, present invention generally provides following technical scheme:A kind of preparation of silicon carbide ceramics precast body Method, comprise the following steps:
The raw material for preparing silicon carbide ceramics precast body is well mixed, raw material slurry is made;Wherein, it is described to prepare carborundum pottery The raw material of porcelain precast body includes carborundum, dispersant, organic monomer and water;The volume of the carborundum and the raw material slurry Than for 40-70:100;
Initiator is added into the raw material slurry, ceramic slurry is obtained after well mixed;Wherein, the initiator and institute The mass ratio for stating raw material slurry is 0.5-5:1000;
Carry out vacuum degassing processing, casting, demoulding drying successively to the ceramic slurry, obtain biscuit of ceramics;
The biscuit of ceramics is sintered at 800-1200 DEG C, obtains silicon carbide ceramics precast body.
The preparation method of foregoing silicon carbide ceramics precast body, the mass ratio of the dispersant and the carborundum are 0.5-1.5:100;The mass ratio of the organic monomer and water is 1:5-1:10.
The preparation method of foregoing silicon carbide ceramics precast body, the organic monomer are acrylamide and di-2-ethylhexylphosphine oxide third The mixture of acrylamide, and the mass ratio of the acrylamide and the methylene-bisacrylamide is 1:3-1:10;
The initiator is azo initiator or ammonium persulfate;
The dispersant is ammoniacal liquor.
The preparation method of foregoing silicon carbide ceramics precast body, the raw material for preparing silicon carbide ceramics precast body also wrap Include pore creating material;
The volume ratio of the pore creating material and the carborundum is 0-1:10;
The pore creating material is the mixture of any of carbon dust, graphite powder or two kinds.
The preparation method of foregoing silicon carbide ceramics precast body, the ceramic slurry is carried out using vacuum degassing tank true Empty degassing processing;
The vacuum of the vacuum degassing processing is 5 × 10-6pa-5 × 10-2pa;
The time of the vacuum degassing processing is 2-20min.
The preparation method of foregoing silicon carbide ceramics precast body, the ceramic slurry after vacuum degassing is injected into non- After punch die, the non-punch die is sealed;
The non-punch die for filling the ceramic slurry is heated to 50-100 DEG C, 100-150min is incubated, is naturally cooling to Room temperature, obtain the ceramic body of solidifying and setting;
After the ceramic body of the solidifying and setting is dried into 12-72 hours in drying box, biscuit of ceramics is obtained.
The preparation method of foregoing silicon carbide ceramics precast body, place is sintered to the biscuit of ceramics using high temperature furnace Reason, the time of the sintering processes is 1-5h.
On the other hand, it is a further object to provide a kind of silicon carbide ceramics precast body, the silicon carbide ceramics Precast body is prepared by the method described in any of the above-described.
On the other hand, it is a further object to provide a kind of preparation method of aluminum-base silicon carbide ceramic material, bag Include following steps:
Silicon carbide ceramics precast body is placed in an open-top receptacle;
Aluminium alloy is covered on the silicon carbide ceramics precast body;Wherein, the aluminium alloy quality is the silicon carbide ceramics The 40-80% of prefabricated weight;
900-1500 DEG C is heated under the atmosphere of nitrogen, by the silicon carbide ceramics precast body and the aluminium alloy, is incubated 1- 5 hours, the aluminium alloy is fully penetrated into the silicon carbide ceramics precast body, aluminum-base silicon carbide ceramic material is made;
Wherein, preparation method system of the silicon carbide ceramics precast body as the silicon carbide ceramics precast body described in any of the above-described It is standby to form.
On the other hand, it is a further object to provide a kind of aluminum-base silicon carbide ceramic material, the aluminium base carbonization The preparation method of silicon ceramic material aluminum-base silicon carbide ceramic material described above is prepared.
Compared with prior art, a kind of silicon carbide ceramics precast body provided by the invention, aluminum-base silicon carbide ceramic material and Its preparation method at least has the advantages that:
The embodiment of the present invention provides a kind of preparation method of silicon carbide ceramics precast body, and the preparation method is gel casting forming Technique, it is specially:Carborundum, dispersant, organic monomer and water are well mixed, so that silicon-carbide particle, organic monomer are homogeneous Ground is dispersed in water;The initiator then added, ceramic slurry (gel) is then subjected to vacuum degassing processing, casting, Make organic monomer polymerize to form macromolecular, and then raw material slurry is formed gel, and silicon-carbide particle is evenly dispersed in gel In, the demoulding dries, obtains silicon carbide ceramics precast body after sintering processes.Above-mentioned preparation method, which can be realized, prepares high volume integral The carborundum precast body of number (volume fraction of carborundum is 40%-70%).Above-mentioned preparation method can make silicon-carbide particle, Pore creating material particle is dispersed in water, forms the particle close-packed structure that size particles are uniformly accumulated, and ceramic slurry is stable Property it is good, for a long time in settled without particle, ensure that in the silicon carbide ceramics precast body obtained by gel injection molding and forming technology big The mutual closs packing of little particle, in the absence of local granule it is overstocked the problems such as, so as to ensure that silicon carbide ceramics precast body microstructure Uniformly, the intensity and knot of aluminum-base silicon carbide composite ceramic material obtained after the pressure-free impregnation aluminium alloy in raising later stage is advantageous to Structure stability.
The carborundum precast body intensity that the embodiment of the present invention is prepared using gel injection molding and forming technology is high, relative to dry-pressing For the moulding process such as shaping, the technique that the embodiment of the present invention uses effectively increases precast body intensity, avoids precast body from removing Destruction during fortune, pressure-free impregnation, and then improve yield rate.
The embodiment of the present invention is a kind of near-net-shape technique using gel injection molding and forming technology, is adapted to prepare big chi Very little, complicated shape product, this point be other existing moulding process it is incomparable.
The preparation method of silicon carbide ceramics precast body provided in an embodiment of the present invention is preparing silicon carbide ceramics precast body When, the content for adding organic monomer is low (being less than 3%), and low content of organics can ensure that silicon carbide ceramics precast body exists The problem of deformation or the cracking of base substrate occurs during high temperature exclusion organic matter;In addition, the use of relatively low organic matter can subtract The small harm to environment.
The preparation method of the silicon carbide ceramics precast body of the embodiment of the present invention is selected when preparing silicon carbide ceramics precast body Azo initiator or ammonium persulfate can trigger having in raw material slurry as acrylamide and the initiator of bisacrylamide Machine monomer (acrylamide and bisacrylamide) slowly polymerize, and solves other initiators and triggers monomer to polymerize and cause rapidly The problem of operating time is short.
Low temperature presintering technique of the embodiment of the present invention, biscuit of ceramics is subjected to pre-sintering, organic matter is excluded with pre- burnt together Two be one, and biscuit of ceramics pre-sintering technology can make final carborundum precast body surface form layer of silicon dioxide film, and then Silicon carbide ceramics precast body is reduced when aluminum-base silicon carbide ceramic material is prepared in the later stage with the surface tension of liquid aluminium alloy, is had Beneficial to being smoothed out for pressureless infiltration process.
In addition, the preparation method of aluminum-base silicon carbide ceramic material provided in an embodiment of the present invention, by by aluminium alloy without pressure Penetrate into the silicon carbide ceramics precast body of above-mentioned preparation, obtain intensity is higher, structure is homogeneous, silicon carbide body fraction is higher, The aluminum-base silicon carbide ceramic material of better performances, and nearly " net " size shaping of aluminum-base silicon carbide ceramics can be realized.
Brief description of the drawings
Fig. 1 is a kind of flow chart of the preparation method of aluminum-base silicon carbide ceramic material provided in an embodiment of the present invention;
Fig. 2 be the embodiment of the present invention prepare biscuit of ceramics pre-sintering handle when, sintering schedule curve map;
Fig. 3 is the schematic diagram provided in an embodiment of the present invention for preparing aluminum-base silicon carbide ceramic material;
Fig. 4 is one embodiment of the invention schematic diagram;
Fig. 5 is a kind of microstructure schematic diagram of silicon carbide ceramics precast body prepared by the embodiment of the present invention;
Fig. 6 is a kind of microstructure schematic diagram of aluminum-base silicon carbide ceramic material prepared by the embodiment of the present invention.
Embodiment
Further to illustrate that the present invention to reach the technological means and effect that predetermined goal of the invention is taken, ties below Preferred embodiment is closed, to according to a kind of silicon carbide ceramics precast body, aluminum-base silicon carbide ceramic material and its system proposed by the present invention Preparation Method embodiment, feature and its effect, describe in detail as follows.
Silicon carbide ceramics precast body is the primary raw material for preparing aluminum-base silicon carbide ceramic material, and silicon carbide ceramics is prefabricated The performance of body is to determine the key factor of aluminum-base silicon carbide ceramic material.And silicon carbide ceramics prepared by existing preparation technology is pre- The performance of body processed is not very well (e.g., the volume fraction of low intensity, structural homogeneity difference and carborundum is low), after influenceing The performance (volume fraction is low, low intensity, can not realize that nearly " net " size is molded) of phase aluminum-base silicon carbide ceramic material.Based on this, The present inventor invents a kind of new preparation method, prefabricated to prepare the silicon carbide ceramics that intensity is higher, structure is homogeneous Body, nearly " net " size shaping, high silicon carbide body fraction, high performance aluminum-base silicon carbide material are prepared so as to realize.
Specifically, the embodiment of the present invention provides a kind of preparation method of silicon carbide ceramics precast body, and this method mainly uses Gel injection molding and forming technology, as shown in figure 1, mainly the preparation including raw material slurry, add initiator into raw material slurry, it is true Empty degasification, injection molding solidify so that monomer be polymerized to macromolecular gel, the demoulding dry, sintering processes step, specifically include as follows:
1) raw material for preparing silicon carbide ceramics precast body is well mixed, raw material slurry is made.Wherein, silicon carbide ceramics is prepared The raw material of precast body includes carborundum, dispersant, organic monomer and water.
In the step, the volume ratio of carborundum and raw material slurry is (40-70):100.The quality of dispersant and carborundum Than for (0.5-2):100.The mass ratio of organic monomer and water is 1:5-1:10.
It is preferred that the carborundum in the step prepares material for the main of ceramics, preferably using that particle diameter is 3-50 μm Grain.The embodiment of the present invention is by selecting suitable silicon-carbide particle grading, dispersant, initiator to realize low viscosity, high stable Property ceramic slurry prepare and high-strength ceramic precast body preparation.
It is preferred that the dispersant in the step is mainly used in being uniformly dispersed silicon carbide ceramics powder, pore creating material particle In raw material slurry, and then it is evenly dispersed in ceramic slurry, biscuit of ceramics and the carborundum finally given of later stage preparation In ceramics preparative body;Preferably, the dispersant in the embodiment of the present invention is preferably ammoniacal liquor, and ammoniacal liquor can make the solid of raw material slurry The suspending power enhancing of particle, do not precipitate, make whole raw material slurry system physico-chemical property the same.
It is preferred that the organic monomer in the step is mainly used in the presence of added initiator in the next step, shape Into macromolecular, and then raw material slurry is set to form gel.It is preferred that organic monomer in the embodiment of the present invention for acrylamide and Mixture in methylene-bisacrylamide.(mass ratio is by a certain percentage for acrylamide monomer and bisacrylamide:1:3- 1:10) mix, the gel for the cross network structure being polymerized in the presence of initiator.
It is preferred that the raw material for preparing silicon carbide ceramics precast body in the step also includes pore creating material;Pore creating material and former carbon The volume ratio of SiClx is (0-1):10.One or more of mixtures that pore creating material is selected in graphite powder, carbon dust, and pore creating material Granularity is 1-10 μm of particle.Here, the main function of pore creating material is used to give silicon carbide ceramics precast body pore-creating, increase is finally The space of the silicon carbide ceramics precast body of preparation, so when the silicon carbide ceramics precast body that the embodiment of the present invention is finally prepared exists During applied to preparing aluminum-base silicon carbide ceramics, it is internally formed porous available for aluminium alloy is accommodated, so as to improve and aluminium and gold Compatibility.
2) initiator is added into raw material slurry, ceramic slurry is obtained after well mixed;Wherein, initiator and raw material The mass ratio of slurry is 0.5-5:1000.
It is preferred that the initiator in the step is preferably azo initiator (e.g., azodiisobutyronitrile (AIBN), azo two Different heptonitrile (ABVN) etc.) or ammonium persulfate.Here, from azo initiator, ammonium persulfate as acrylamide and double acryloyls The initiator of amine, the organic monomer (acrylamide and bisacrylamide) in raw material slurry can be triggered slowly to polymerize, solved The problem of other initiators trigger rapidly monomer to polymerize and cause the operating time short.
In addition, the mass ratio of the initiator and the raw material slurry in the step is preferably 1:1000.
3) after handling ceramic slurry vacuum degassing, it is injection molded, biscuit of ceramics is obtained after drying.Specifically include:
31) ceramic slurry is put into vacuum degassing tank, opens vavuum pump, keep the vacuum in vacuum degassing tank for 5 × 10-6Pa-5 × 10-2Pa, vacuum degassing 2-20min;
The step is mainly used in fully removing the bubble in silicon carbide slurry, avoids drawing in the biscuit of ceramics that casting obtains Enter hole of holding one's breath, so as to influence material density.
32) after the ceramic slurry after vacuum degassing is handled is injected in non-punch die, non-punch die is sealed, makes non-hole Ceramic slurry in mould is in closed state;Non- punch die is placed and is heated to 50-80 DEG C in an oven, and is incubated extremely After 100-150min, Temperature fall, make the ceramic slurry curing molding in non-punch die, obtain the ceramic body of curing molding (that is, biscuit of ceramics).
The material of non-punch die in the step can be metal, glass, plastics;According further to the shape of non-punch die Ceramic slurry curing molding can be different shape (such as tabular, strip) by difference.
33) ceramic body (that is, biscuit of ceramics) of curing molding is placed in drying box after the taking-up of non-punch die After drying 12-72 hours (preferably 36 hours), dry biscuit of ceramics is obtained.
4) biscuit of ceramics is sintered at 800-1200 DEG C, obtains aluminum-base silicon carbide ceramics preparative body.
The step is specially:Biscuit of ceramics is placed in high temperature furnace, it is natural after being incubated 1-5h at 800-1200 DEG C Cooling, obtains high intensity aluminum-base silicon carbide ceramics preparative body.
The step is by the way that biscuit of ceramics is sintered, it is possible to achieve following purpose:First, the embodiment of the present invention With low temperature presintering technique, biscuit of ceramics is subjected to pre-sintering, organic matter is excluded to be combined into one with pre-burning;Second, make ceramic element Pore creating material in base carries out burning mistake, so as to generate porous aluminum-base silicon carbide ceramics preparative body, and then makes the aluminium base carbonized ceramic Precast body enables aluminum alloy to be contained in porous, it is prefabricated to add aluminium base carbonized ceramic when preparing aluminium base carbonized ceramic precast body The compatibility of body and aluminium alloy;3rd, layer of silicon dioxide film can be formed in aluminium base carbonized ceramic precast body surface, reduced Aluminium base carbonized ceramic precast body is advantageous to being smoothed out for infiltration process with the surface tension of liquid aluminium alloy;4th, can be with The intensity of aluminium base carbonized ceramic precast body is effectively improved, reduces aluminium base carbonized ceramic precast body because of the possibility destroyed by external force Property, improve yield rate.When biscuit of ceramics is sintered in high temperature furnace, the change of temperature over time is as shown in Fig. 2.
To sum up, silicon carbide ceramics precast body gel injection molding and forming technology provided in an embodiment of the present invention is a kind of novel-section Expect technology of preparing, this method is by the preparation of low viscosity raw material slurry, casting, hot setting is shaped, the demoulding is dried, high temperature Degreasing sintered acquisition high intensity, low viscosity silicon carbide ceramics precast body.The embodiment of the present invention solves low viscosity ceramic slurry system Standby problem, controllable cured sizing problem, the degreasing sintered problem of high temperature, high-strength carborundum ceramics preparative body can be achieved and prepare.
In addition, the embodiment of the present invention also provides a kind of preparation method of aluminum-base silicon carbide ceramic material, this method is mainly wrapped Include following steps:
1) silicon carbide ceramics precast body is placed in an open-top receptacle.
2) aluminium alloy is placed on silicon carbide ceramics precast body;Wherein, the aluminium alloy quality is made pottery for the carborundum The 40-80% of the prefabricated weight of porcelain;
3) 900-1200 DEG C is heated under the atmosphere of nitrogen, by silicon carbide ceramics precast body and aluminium alloy, is incubated 1-5 hours, Enable aluminum alloy to fully penetrate into silicon carbide ceramics precast body, aluminum-base silicon carbide ceramic material is made.
Specifically, the open-top receptacle in the step is heat-resisting and not reacted with silicon carbide ceramics precast body, aluminium alloy Container, the embodiment of the present invention preferably uses corundum crucible.As shown in figure 3, carborundum precast body 1 is placed on corundum crucible 2 It is interior;Aluminium alloy 3 is placed on silicon carbide ceramics precast body 1 again;In a nitrogen atmosphere, by silicon carbide ceramics precast body and aluminium Alloy is heated to 900-1200 DEG C (preferably 1100 DEG C), insulation 1-5 hours (preferably 2 hours), treats that aluminium alloy is fully penetrated into carbon In SiClx ceramics preparative body, aluminum-base silicon carbide ceramic material is made.Wherein, silicon carbide ceramics precast body and aluminium alloy soak without pressure It is as shown in Figure 4 to ooze temperature profile.
In addition, the embodiment of the present invention also provides a kind of aluminum-base silicon carbide ceramic material, the aluminum-base silicon carbide ceramic material by The preparation method of above-mentioned aluminum-base silicon carbide ceramic material is prepared.
The present invention is described in further detail with reference to the accompanying drawings and examples.
The raw material used and density in following examples are:Silicon-carbide particle (density 3.21g/cm3);Ammoniacal liquor (25% solution, density 0.91);Carbon dust, graphite powder (density 2.2g/cm3).Ammonium persulfate, acrylamide, di-2-ethylhexylphosphine oxide Acrylamide is that analysis is pure.
Embodiment 1
A kind of carborundum precast body of 65% volume fraction is prepared (here, 65% volume fraction refers to that carborundum is pre- in carborundum Shared volume fraction in body processed, below similarly);Comprise the following steps that:
1st, by 208.6 grams, silicon-carbide particle, 4 grams of acrylamide monomers, the 1 gram of methylene bisacrylamide acyl that granularity is 3-20 microns Amine, 30 grams of water, 2 grams of ammoniacal liquor are added in agitator tank, and stirring obtains raw material slurry after 24 hours.
2nd, the different cyanogen in heptan of 1.2 grams of azos two is added in raw material slurry, stirring obtains ceramic slurry after 30 minutes.
3rd, ceramic slurry is placed in vacuum degassing tank, vacuum degassing is carried out to ceramic slurry;Wherein, remove vacuum Vacuum in gas tank is maintained at 5 × 10-2Pa, and the vacuum degassed time is 5 minutes.
4th, the ceramic slurry after vacuum degassing is injected in non-punch die, and it is small to be placed into insulation 3 in 70 DEG C of baking oven When, make ceramic slurry solidifying and setting, then be placed into dry phase and dry 36 hours, obtain biscuit of ceramics.
5th, biscuit of ceramics is placed into high temperature furnace, is warming up to 1100 DEG C, after being incubated 2 hours, Temperature fall, obtain height The silicon carbide ceramics precast body of intensity.
Embodiment 2
Prepare a kind of carborundum precast body of 60% volume fraction;Comprise the following steps that:
1st, it is 10 microns of silicon-carbide particle, 66 grams of carbon dust, 40 grams of acrylamide monomers, 10 grams of methylenes by 1926 grams, granularity Base bisacrylamide, 320 grams of water, 19 grams of ammoniacal liquor are added in agitator tank, and stirring obtains raw material slurry after 24 hours.
2nd, the different cyanogen in heptan of 11 grams of azos two is added in raw material slurry, stirring obtains ceramic slurry after 30 minutes.
3rd, ceramic slurry is placed in vacuum degassing tank, vacuum degassing is carried out to ceramic slurry;Wherein, remove vacuum Vacuum in gas tank is maintained at 5 × 10-6Pa, and the vacuum degassed time is 5 minutes.
4th, the ceramic slurry after vacuum degassing is injected in non-punch die, and it is small to be placed into insulation 3 in 70 DEG C of baking oven When, make ceramic slurry solidifying and setting, then be placed into dry phase and dry 36 hours, obtain biscuit of ceramics.
5th, biscuit of ceramics is placed into high temperature furnace, is warming up to 1100 DEG C, after being incubated 2 hours, Temperature fall, obtain height The silicon carbide ceramics precast body of intensity.
Embodiment 3
Prepare a kind of carborundum precast body of 57% volume fraction;Comprise the following steps that:
1st, it is 20 microns of silicon-carbide particle, 20 grams of graphite powders, 36 grams of acrylamide monomers, 4 grams of methylene by 800 grams, granularity Bisacrylamide, 150 grams of water, 16 grams of ammoniacal liquor are added in agitator tank, and stirring obtains raw material slurry after 24 hours.
2nd, 5 grams of ammonium persulfates are added in raw material slurry, stirring obtains ceramic slurry after 30 minutes.
3rd, ceramic slurry is placed in vacuum degassing tank, vacuum degassing is carried out to ceramic slurry;Wherein, remove vacuum Vacuum in gas tank is maintained at 5 × 10-4Pa, and the vacuum degassed time is 5 minutes.
4th, the ceramic slurry after vacuum degassing is injected in non-punch die, and it is small to be placed into insulation 3 in 70 DEG C of baking oven When, make ceramic slurry solidifying and setting, then be placed into dry phase and dry 36 hours, obtain biscuit of ceramics.
5th, biscuit of ceramics is placed into high temperature furnace, is warming up to 1100 DEG C, after being incubated 2 hours, Temperature fall, obtain height The silicon carbide ceramics precast body of intensity.
Embodiment 4
Prepare a kind of carborundum precast body of 70% volume fraction;Comprise the following steps that:
1st, by 290 grams, granularity be 30 microns silicon-carbide particle, 4 grams of acrylamide monomers, 1 gram of methylene-bisacrylamide, 33 grams of water, 2 grams of ammoniacal liquor are added in agitator tank, and stirring obtains raw material slurry after 24 hours.
2nd, the different cyanogen in heptan of 1.2 grams of azos two is added in raw material slurry, stirring obtains ceramic slurry after 30 minutes.
3rd, ceramic slurry is placed in vacuum degassing tank, vacuum degassing is carried out to ceramic slurry;Wherein, remove vacuum Vacuum in gas tank is maintained at 5 × 10-2Pa, and the vacuum degassed time is 5 minutes.
4th, the ceramic slurry after vacuum degassing is injected in non-punch die, and it is small to be placed into insulation 3 in 70 DEG C of baking oven When, make ceramic slurry solidifying and setting, then be placed into dry phase and dry 36 hours, obtain biscuit of ceramics.
5th, biscuit of ceramics is placed into high temperature furnace, is warming up to 1100 DEG C, after being incubated 2 hours, Temperature fall, obtain height The silicon carbide ceramics precast body of intensity.
Test the intensity of the silicon carbide ceramics precast body of the preparation of embodiment 1- embodiments 4 respectively using three-point bending method, Test result is as shown in table 1.
Table 1
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4
Bending strength(MPa) 27 25 22 29
As it can be seen from table 1 the intensity of silicon carbide ceramics precast body prepared by the embodiment of the present invention is higher, adopted far above existing The intensity of the silicon carbide ceramics precast body prepared with dry pressing, injection moulding (less than 15MPa).
The microstructure of silicon carbide ceramics precast body prepared by embodiment 1- embodiments 4 using electron microscope observation, Wherein, the microstructure of silicon carbide ceramics precast body prepared by embodiment 1 is as shown in Figure 5.As can be seen that the embodiment of the present invention The microstructure of the silicon carbide ceramics precast body of preparation is homogeneous, i.e., silicon carbide ceramics uniformly combines in the presence of gel network Together, here it is silicon carbide ceramics precast body to have the main reason for high intensity.And silicon carbide ceramics precast body is high-strength Degree, homogeneous microstructure are the preconditions for preparing high-performance aluminium-base thyrite.
Embodiment 5
Silicon carbide ceramics precast body prepared by embodiment 1 is placed in the first corundum crucible;Carbonization prepared by embodiment 2 Silicon ceramics preparative body is placed in the second corundum crucible;It is firm that silicon carbide ceramics precast body prepared by embodiment 3 is placed on the 3rd In beautiful crucible;Silicon carbide ceramics precast body prepared by embodiment 4 is placed in the 4th corundum crucible.Respectively to the first corundum Aluminium alloy is heated in crucible, the second corundum crucible, the 3rd corundum crucible and the 4th corundum crucible, enables aluminum alloy to cover carborundum Ceramics preparative body.Then the first corundum crucible, the second corundum crucible, the 3rd corundum crucible and the 4th corundum crucible are placed on In high temperature furnace, 1100 DEG C are heated to, and 2 hours are incubated at 1100 DEG C, enables aluminum alloy to fully penetrate into prefabricated to silicon carbide ceramics Body, after naturally cooling to room temperature, respectively obtain (the aluminium base carbonization that wherein, the first crucible obtains of aluminum-base silicon carbide ceramic material Silicon ceramic material is designated as the first aluminum-base silicon carbide ceramic material;The aluminum-base silicon carbide ceramic material that second crucible obtains is designated as Two aluminum-base silicon carbide ceramic materials;The aluminum-base silicon carbide ceramic material that 3rd crucible obtains is designated as the 3rd aluminum-base silicon carbide ceramics Material;The aluminum-base silicon carbide ceramic material that 4th crucible obtains is designated as the 4th aluminum-base silicon carbide ceramic material).
Aluminium alloy used includes following composition in the present embodiment:Mg contents are 3%, Si contents are 0.7%, and remaining is Al。
Test the first aluminum-base silicon carbide ceramic material manufactured in the present embodiment, the second aluminium respectively using three-point bending method The intensity of base silicon carbide ceramic material, the 3rd aluminum-base silicon carbide ceramic material and the 4th aluminum-base silicon carbide ceramic material, test knot Fruit is as shown in table 2, and the first aluminum-base silicon carbide ceramic material microstructure photograph is as shown in Fig. 6.
Table 2
Bending strength(MPa)
First aluminum-base silicon carbide ceramic material 340
Second aluminum-base silicon carbide ceramic material 317
3rd aluminum-base silicon carbide ceramic material 280
4th aluminum-base silicon carbide ceramic material 330
From table 2 it can be seen that the intensity of aluminum-base silicon carbide ceramic material prepared by the embodiment of the present invention is higher, far above existing The aluminum-base silicon carbide ceramic material that the silicon carbide ceramics precast body for using dry pressing, injection moulding to prepare is prepared for raw material Intensity.
To sum up, silicon carbide ceramics precast body provided in an embodiment of the present invention realize prepare high-volume fractional (carborundum Volume fraction is 40%-70%), even microstructure, high intensity carborundum precast body, be advantageous to improve the later stage without pressure The intensity and structural stability of the aluminum-base silicon carbide composite ceramic material obtained after infiltration aluminium alloy.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, and appoints What those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, all should It is included within the scope of the present invention.Therefore, protection scope of the present invention should using the scope of the claims as It is accurate.

Claims (10)

1. a kind of preparation method of silicon carbide ceramics precast body, it is characterised in that comprise the following steps:Silicon carbide ceramics will be prepared The raw material of precast body is well mixed, and raw material slurry is made;Wherein, the raw material for preparing silicon carbide ceramics precast body includes carbon SiClx, dispersant, organic monomer and water;The volume ratio of the carborundum and the raw material slurry is 40-70:100;It will trigger Agent is added into the raw material slurry, and ceramic slurry is obtained after well mixed;Wherein, the initiator and the raw material slurry Mass ratio be 0.5-5:1000;Carry out vacuum degassing processing, casting, demoulding drying successively to the ceramic slurry, obtain To biscuit of ceramics;The biscuit of ceramics is sintered at 800-1200 DEG C, obtains silicon carbide ceramics precast body.
2. the preparation method of silicon carbide ceramics precast body according to claim 1, it is characterised in that the dispersant and institute The mass ratio for stating carborundum is 0.5-2:100;The mass ratio of the organic monomer and water is 1:5-1:10.
3. the preparation method of silicon carbide ceramics precast body according to claim 2, it is characterised in that the organic monomer is The mixture of acrylamide and methylene-bisacrylamide, and the matter of the acrylamide and the methylene-bisacrylamide Amount is than being 3:1-10:1;The initiator is azo initiator or ammonium persulfate;The dispersant is ammoniacal liquor.
4. the preparation method of the silicon carbide ceramics precast body according to claim any one of 1-3, it is characterised in that described Preparing the raw material of silicon carbide ceramics precast body also includes pore creating material;The volume ratio of the pore creating material and the carborundum is 0-1: 10;The pore creating material is the mixture of any of carbon dust, graphite powder or two kinds.
5. the preparation method of silicon carbide ceramics precast body according to claim 1, it is characterised in that using vacuum degassing tank Vacuum degassing processing is carried out to the ceramic slurry;The vacuum of the vacuum degassing processing is 5 × 10-6pa-5 × 10-2pa; The time of the vacuum degassing processing is 2-20min.
6. the preparation method of silicon carbide ceramics precast body according to claim 1, it is characterised in that vacuum degassing will be passed through After ceramic slurry afterwards is injected into non-punch die, the non-punch die is sealed;The non-hole of the ceramic slurry will be filled Mould is heated to 50-80 DEG C, is incubated 100-150min, is naturally cooling to room temperature, obtains the ceramic body of solidifying and setting;By institute The ceramic body for stating solidifying and setting after dry 12-72 hours, obtains biscuit of ceramics in drying box.
7. the preparation method of silicon carbide ceramics precast body according to claim 1, it is characterised in that using high temperature furnace pair The biscuit of ceramics is sintered, and the time of the sintering processes is 1-5h.
8. a kind of silicon carbide ceramics precast body, it is characterised in that the silicon carbide ceramics precast body is any by claim 1-7 Method described in is prepared.
9. a kind of preparation method of aluminum-base silicon carbide ceramic material, it is characterised in that comprise the following steps:Silicon carbide ceramics is pre- Body processed is placed in an open-top receptacle;Aluminium alloy is covered on the silicon carbide ceramics precast body;Wherein, the aluminium alloy matter Measure as the 40-80% of the prefabricated weight of the silicon carbide ceramics;Under the atmosphere of nitrogen, by the silicon carbide ceramics precast body 900-1200 DEG C is heated to the aluminium alloy, is incubated 1-5 hours, the aluminium alloy is fully penetrated into the carborundum pottery In porcelain precast body, aluminum-base silicon carbide ceramic material is made;Wherein, the silicon carbide ceramics precast body is any by claim 1-7 The preparation method of silicon carbide ceramics precast body described in is prepared.
10. a kind of aluminum-base silicon carbide ceramic material, it is characterised in that the aluminum-base silicon carbide ceramic material is by claim 9 institute The preparation method for the aluminum-base silicon carbide ceramic material stated is prepared.
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CN112739664A (en) * 2018-09-28 2021-04-30 福吉米株式会社 Coated silicon carbide particle powder
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CN114702317A (en) * 2022-03-24 2022-07-05 湖南太子新材料科技有限公司 Low-temperature sintering method of high-performance silicon carbide ceramic material
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